Several chemical processes of utmost industrial relevance occur at
medium/elevated pressure of gases, for example many Ziegler-Natta
polymerizations, and almost all hydrogenation and carbonylation reactions
of unsaturated substrates. The investigations in these fields are commonly
carried out in autoclaves that are generally expensive and devoid of many
devices of importance to control and monitor the course of the reactions.
Also, a high gas pressure does not allow for in situ studies of the
reactions by means of standard spectroscopic techniques, which may limit
the understanding of many processes as well as their
improvement/optimization. The research laboratories looking for excellence
are therefore obliged to design and construct this kind of scientific
instrumentation.
The activity at the ICCOM in the area of catalytic technologies under
elevated gas pressure is advanced, known worldwide and a primary source of
financial income. In order to achieve these results and maintain a lasting
level of excellence, the mechanical and electronic workshop of the
Institute carries out an intense activity in the design and construction
of high pressure devices for spectroscopic measurements.
Nowadays, the ICCOM is an advanced center for the development of the
following instrumentation:
- high-pressure reactors (up to 250 bar and 250 °C) equipped with
solid and liquid injectors, sampling devices, controllers of temperature,
stirring rate and pressure. The picture of a standard autoclave
constructed at ICCOM is shown in Figure 1.
- high-pressure NMR tubes (up to 250 bar and 200 °C) constituted by
10 mm OD sapphire tubes sealed by amagnetic titanium valves, comprising
high-temperature rotors, charging systems for gases, and pliers for the
introduction of the tubes into the spectrometer probehead (Figure 2).
- IR cells for the continuous monitoring of high-pressure reactions
carried out in autoclaves.
The capability to follow the same chemical process with two distinct
spectroscopic techniques working at different time scale such as NMR and
IR allows for the obtainment of valuable mechanistic and kinetic
information.
The demand of the high-pressure instrumentation developed at ICCOM is so
great to forecast the creation of a spin-off enterprise with good chances
of success.
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